CN108913884A - Low alkali high temperature and pressure decomposes the method that wolframite prepares coarse sodium tungstate - Google Patents
Low alkali high temperature and pressure decomposes the method that wolframite prepares coarse sodium tungstate Download PDFInfo
- Publication number
- CN108913884A CN108913884A CN201810813445.XA CN201810813445A CN108913884A CN 108913884 A CN108913884 A CN 108913884A CN 201810813445 A CN201810813445 A CN 201810813445A CN 108913884 A CN108913884 A CN 108913884A
- Authority
- CN
- China
- Prior art keywords
- wolframite
- slurry
- pressure
- sodium
- sodium tungstate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/12—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic alkaline solutions
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/36—Obtaining tungsten
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Geology (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a kind of low alkali high temperature and pressure to decompose the method that wolframite prepares coarse sodium tungstate, includes the following steps：Wolframite powder and water are mixed to form wolframite slurry, sodium hydroxide, tertiary sodium phosphate, sodium nitrate is sequentially added into wolframite slurry size mixing forming wolframite mixing slurry, wolframite mixing slurry is decomposed, decomposition temperature is 192~210 DEG C, pressure is 0.8~1.0MPa, it is diluted after decomposition, filters pressing, washing, takes filtrate, obtain coarse sodium tungstate, wherein, the additional amount of sodium hydroxide is 1.4~1.6 times by the theoretical amount of tungstic acid weight in wolframite powder.The present invention has the beneficial effect for reducing base amount, improving wolframite tungsten resolution ratio.
Description
Technical field
The present invention relates to Tungsten smelting fields.It is more particularly related to which a kind of low alkali high temperature and pressure decomposes black tungsten essence
The method that mine prepares coarse sodium tungstate.
Background technique
China's wolframite smelting process experienced three developing stage：First stage, the Soviet Union introduced from the Soviet Union in 1958
Beat sintering (decompose afterwards for sodium hydroxide) → purification and impurity removal → sink white tungsten → acid decomposition → ammonia it is molten → evaporative crystallization production para-tungstic acid
The classical technique of ammonium (APT), since technique is long, the defective workmanships such as metal recovery rate is low, seriously corroded, poor product quality are classical
Technique essentially drops out production field at the beginning of nineteen ninety；Second stage, 1981, black tungsten autoclaving → purification and impurity removal → extraction → evaporation
The extraction process of crystallization production APT puts into production in Zhuzhou Hard Alloy Plant；Phase III, the pioneering ion of nineteen eighty-three China are handed over
It changes technique to be born in Zhuzhou tungsten and molybdenum material factory, since process flow is short, metal high income, product quality and environmental condition are good, behaviour
Make the series of advantages such as simple, is just rapidly developed since being born.Currently, application surface has accounted for the 90% of Tungsten smelting industry, at
For the mainstream process of China APT production, coarse sodium tungstate is the primary raw material for producing APT.
Existing tungsten smelting process mainly passes through sodium hydroxide Decomposition of Tungsten and obtains coarse sodium tungstate, although entire technique is
One mature technique, but part producing enterprise is excessive using upper consumption in auxiliary material sodium hydroxide, sodium hydroxide concentration reaches
2.5~3.0 times of theoretical decomposition amount, cause remaining sodium hydroxide excessive, therefore subsequent coarse sodium tungstate carries out ion exchange
Before, needing to consume a large amount of water dilution coarse sodium tungstates can just make naoh concentration be less than 8g/L, and wastewater treatment is caused to work
Amount increases, and the production cost increases.
Summary of the invention
It is an object of the invention to solve at least the above problems, and provide the advantages of at least will be described later.
Wolframite, which is decomposed, it is a still further object of the present invention to provide a kind of alkali high temperature and pressure prepares coarse sodium tungstate
Method considerably reduces base amount, improves wolframite tungsten resolution ratio, reduces enterprise's production cost.
In order to realize these purposes and other advantages according to the present invention, a kind of black tungsten of low alkali high temperature and pressure decomposition is provided
The method that concentrate prepares coarse sodium tungstate, includes the following steps：Wolframite powder and water are mixed to form wolframite slurry, to black
Sodium hydroxide, tertiary sodium phosphate, sodium nitrate are sequentially added in tungsten ore slurry to carry out sizing mixing to form wolframite mixing slurry, and wolframite is mixed
Slurry is decomposed, and decomposition temperature is 192~210 DEG C, pressure is 0.8~1.0MPa, is diluted, filters pressing, washing, takes after decomposition
Filtrate obtains coarse sodium tungstate, wherein the additional amount of sodium hydroxide is the theory by tungstic acid weight in wolframite powder
1.4~1.6 times of amount.
Preferably, the particle weight accounting that granularity is not less than 325 mesh in wolframite slurry is more than or equal to 96%.
Preferably, the concentration of sodium hydroxide is 175~200g/L in wolframite mixing slurry, the concentration of tertiary sodium phosphate is 20
~65g/L, sodium nitrate concentration be 5~10g/L.
Preferably, mixing speed control is 70~75r/min, 3~4h of heat-insulation pressure keeping in decomposable process.
Preferably, it is diluted the specific steps are：Into dilution trap, note 1/3 dilutes the water of sump volume, after then decomposing
Wolframite mixing slurry import dilution trap in.
Preferably, time of filter pressing is 25~30min, and the temperature of slurry is 50~60 DEG C.
Preferably, the preparation method of wolframite powder is：Choose the wolframite and low calcium content of high calcium content
Wolframite arranges in pairs or groups to form the wolframite that total calcium content is not more than 2%, takes wolframite to be broken into wolframite particle, will surpass
Carefully flour mill is formed closed circuit with screening machine, is taken wolframite particle to be added in superfine mill and is milled, uses solid material
Delivery pump is delivered in screening machine and is sieved, and screenings flows into pulp tank when oversize accumulation is more from diversion trench and will sieve
Oversize is imported superfine mill from diversion trench by the compass screen surface inclination of machine, and after screening, dodecyl is added into pulp tank
Benzene sulfonic acid sodium salt, polyglyceryl fatty acid ester, ethyl alcohol, water, ultrasound, filter to take filter residue, dry, obtain wolframite powder, wherein 12
Sodium alkyl benzene sulfonate, polyglyceryl fatty acid ester, ethyl alcohol, water volume ratio be 1:2:15:100, after decomposing in dilution
Wolframite mixing slurry import dilution trap after be additionally added dilution, from dilution trench bottom be passed through 400~500mL/min of nitrogen,
It is extracted, is vibrated, stratification with ethyl acetate again, remove organic layer solution, filters pressing is carried out to water layer solution, wherein dilute
Releasing liquid includes：Propylene glycol alkyl ether acetic acid ester, dodecyl alcohol polyoxyethylene ether sodium sulfate, dodecyl trimethyl ammonium bromide,
Methyl 2- hydroxy-isobutyric acid ester, 3- methoxy methyl propionate, 1- methoxy-2-propanol ester, ethyl acetate, water, wherein propylene glycol
Alkylether acetates, dodecyl alcohol polyoxyethylene ether sodium sulfate, dodecyl trimethyl ammonium bromide, methyl 2- hydroxy-iso-butyric acid
Ester, 3- methoxy methyl propionate, 1- methoxy-2-propanol ester, ethyl acetate, water volume ratio be 1:2:2:1:2:15:50.
The present invention is include at least the following beneficial effects：
The first, the compound of calcium is mainly artificial schellite in wolframite, since the balance that sodium hydroxide decomposes artificial schellite is normal
Number is smaller, and the high wolframite of calcic just easily decomposes under the conditions of higher alkali concentration, phosphate-containing in wolframite slurry of the present invention,
The thermodynamic driving force for decomposing artificial schellite in wolframite increases, and the calcium obtained after decomposition is reacted with phosphate anion generates solubility
The calcium phosphate of very little not only avoids calcium ion that back reaction occurs and generates white tungsten, but also reduces the dosage of alkali, and sodium hydroxide adds
Entering amount is by 1.4~1.6 times of the theoretical amount of tungstic acid weight in wolframite, since coarse sodium tungstate is carrying out ion
Before exchange, need to make the concentration of the alkali in solution to be less than 8g/L, the dosage for reducing alkali can reduce dilution coarse sodium tungstate water
Dosage, thus reduce coarse sodium tungstate carry out ion exchange after generated waste water amount, reduce cost for wastewater treatment；
The second, it in decomposable process, takes high temperature and pressure measure that tungsten mineral is promoted to decompose, is diluted after decomposition and fastly
Ram compression filter washing, this method decomposition wolframite resolution ratio is higher, and the content of tungstic acid is lower in filter residue, improves tungsten ore
Recovery rate；
Superfine mill and screening machine are formed closed circuit processing wolframite by third, realize automation, reduce manual operation
Process, accelerate process velocity, wolframite powder is through neopelex, polyglyceryl fatty acid ester, ethyl alcohol, water process
It obtains, the adsorbable organic matter with anion, cation of anionic surfactant, cationic surfactant, while will have
Machine object is dispersed in water, alcohol soluble organic matter, in dilution by after decomposition wolframite mixing slurry import dilution trap it
After be additionally added dilution, be passed through 400~500mL/min of nitrogen from dilution trench bottom, then extracted with ethyl acetate, further
The organic substance contained in mine is handled, the impurity of coarse sodium tungstate is reduced.
Further advantage, target and feature of the invention will be partially reflected by the following instructions, and part will also be by this
The research and practice of invention and be understood by the person skilled in the art.
Specific embodiment
The present invention will be further described in detail below with reference to the embodiments, to enable those skilled in the art referring to specification
Text can be implemented accordingly.
It should be noted that experimental method described in following embodiments is unless otherwise specified conventional method, institute
Reagent and material are stated, unless otherwise specified, is commercially obtained.
<Embodiment 1>
Low alkali high temperature and pressure decomposes the method that wolframite prepares coarse sodium tungstate, includes the following steps：Wolframite
Powder and water are mixed to form wolframite slurry, sequentially add sodium hydroxide, tertiary sodium phosphate, sodium nitrate into wolframite slurry and size mixing
Wolframite mixing slurry is formed, wolframite mixing slurry is decomposed, decomposition temperature is 192 DEG C, pressure 0.8MPa, is decomposed laggard
Row dilution, filters pressing, washing, take filtrate, obtain coarse sodium tungstate, and the content of sodium tungstate is 120~160g/ in coarse sodium tungstate
L, wherein the additional amount of sodium hydroxide is 1.4 times by the theoretical amount of tungstic acid weight in wolframite；
Granularity is not less than the particle weight accounting 96% of 325 mesh in wolframite slurry；
The concentration of sodium hydroxide is 175g/L in wolframite mixing slurry, the concentration of tertiary sodium phosphate is 20g/L, sodium nitrate it is dense
Degree is 5g/L；
Mixing speed control is 70r/min, heat-insulation pressure keeping 3h in decomposable process；
It is diluted the specific steps are：Into dilution trap, note 1/3 dilutes the water of sump volume, then mixes the wolframite after decomposition
Slurry is closed to import in dilution trap；
Time of filter pressing is 25min, and the temperature of slurry is 50 DEG C.
<Embodiment 2>
Low alkali high temperature and pressure decomposes the method that wolframite prepares coarse sodium tungstate, includes the following steps：Wolframite
Powder and water are mixed to form wolframite slurry, sequentially add sodium hydroxide, tertiary sodium phosphate, sodium nitrate into wolframite slurry and size mixing
Wolframite mixing slurry is formed, wolframite mixing slurry is decomposed, decomposition temperature is 210 DEG C, pressure 1.0MPa, is decomposed laggard
Row dilution, filters pressing, washing, take filtrate, obtain coarse sodium tungstate, and the content of sodium tungstate is 120~160g/ in coarse sodium tungstate
L, wherein the additional amount of sodium hydroxide is 1.6 times by the theoretical amount of tungstic acid weight in wolframite；
Granularity is not less than the particle weight accounting 98% of 325 mesh in wolframite slurry；
The concentration of sodium hydroxide is 200g/L in wolframite mixing slurry, the concentration of tertiary sodium phosphate is 65g/L, sodium nitrate it is dense
Degree is 10g/L；
Mixing speed control is 75r/min, heat-insulation pressure keeping 4h in decomposable process；
It is diluted the specific steps are：Into dilution trap, note 1/3 dilutes the water of sump volume, then mixes the wolframite after decomposition
Slurry is closed to import in dilution trap；
Time of filter pressing is 30min, and the temperature of slurry is 60 DEG C.
<Embodiment 3>
Low alkali high temperature and pressure decomposes the method that wolframite prepares coarse sodium tungstate, includes the following steps：Wolframite
Powder and water are mixed to form wolframite slurry, sequentially add sodium hydroxide, tertiary sodium phosphate, sodium nitrate into wolframite slurry and size mixing
Wolframite mixing slurry is formed, wolframite mixing slurry is decomposed, decomposition temperature is 200 DEG C, pressure 0.9MPa, is decomposed laggard
Row dilution, filters pressing, washing, take filtrate, obtain coarse sodium tungstate, and the content of sodium tungstate is 120~160g/ in coarse sodium tungstate
L, wherein the additional amount of sodium hydroxide is 1.5 times by the theoretical amount of tungstic acid weight in wolframite；
Granularity is not less than the particle weight accounting 97% of 325 mesh in wolframite slurry；
The concentration of sodium hydroxide is 185g/L in wolframite mixing slurry, the concentration of tertiary sodium phosphate is 40g/L, sodium nitrate it is dense
Degree is 8g/L；
Mixing speed control is 72r/min, heat-insulation pressure keeping 3.5h in decomposable process；
It is diluted the specific steps are：Into dilution trap, note 1/3 dilutes the water of sump volume, then mixes the wolframite after decomposition
Slurry is closed to import in dilution trap；
Time of filter pressing is 28min, and the temperature of slurry is 55 DEG C.
<Embodiment 4>
Low alkali high temperature and pressure decomposes the method that wolframite prepares coarse sodium tungstate, includes the following steps：Wolframite
Powder and water are mixed to form wolframite slurry, sequentially add sodium hydroxide, tertiary sodium phosphate, sodium nitrate into wolframite slurry and size mixing
Wolframite mixing slurry is formed, wolframite mixing slurry is decomposed, decomposition temperature is 200 DEG C, pressure 0.9MPa, is decomposed laggard
Row dilution, filters pressing, washing, take filtrate, obtain coarse sodium tungstate, and the content of sodium tungstate is 120~160g/ in coarse sodium tungstate
L, wherein the additional amount of sodium hydroxide is 1.5 times by the theoretical amount of tungstic acid weight in wolframite；
Granularity is not less than the particle weight accounting 97% of 325 mesh in wolframite slurry；
The concentration of sodium hydroxide is 185g/L in wolframite mixing slurry, the concentration of tertiary sodium phosphate is 40g/L, sodium nitrate it is dense
Degree is 8g/L；
Mixing speed control is 72r/min, heat-insulation pressure keeping 3.5h in decomposable process；
It is diluted the specific steps are：Into dilution trap, note 1/3 dilutes the water of sump volume, then mixes the wolframite after decomposition
Slurry is closed to import in dilution trap；
Time of filter pressing is 28min, and the temperature of slurry is 55 DEG C；
The preparation method of wolframite powder is：The wolframite of the wolframite and low calcium content of choosing high calcium content is taken
With formed total calcium content be not more than 2% wolframite, take wolframite to be broken into wolframite particle, by superfine mill with
Screening machine forms closed circuit, and wolframite is taken to be broken into wolframite particle, superfine mill is formed with screening machine closed circuit, takes black
Tungsten concentrate particle, which is added in superfine mill, to be milled, and is delivered in screening machine and is sieved with solid material delivery pump,
Screenings flows into pulp tank from diversion trench, when oversize accumulation is more, by the inclination of the compass screen surface of screening machine by oversize from diversion trench
Import superfine mill, after screening, into pulp tank be added neopelex, polyglyceryl fatty acid ester, ethyl alcohol,
Water, ultrasound, filter to take filter residue, dry, obtain wolframite powder, wherein neopelex, polyglyceryl fatty acid ester,
Ethyl alcohol, water volume ratio be 1:2:15:100；
The wolframite mixing slurry after decomposition is imported after dilution trap in dilution and is additionally added dilution, from dilution trap bottom
Portion is passed through nitrogen 450mL/min, then is extracted with ethyl acetate, oscillation, and stratification removes organic layer solution, to water layer
Solution carries out filters pressing, wherein dilution includes：Propylene glycol alkyl ether acetic acid ester, dodecyl alcohol polyoxyethylene ether sodium sulfate, ten
Dialkyl group trimethylammonium bromide, methyl 2- hydroxy-isobutyric acid ester, 3- methoxy methyl propionate, 1- methoxy-2-propanol ester, acetic acid
Ethyl ester, water, wherein propylene glycol alkyl ether acetic acid ester, dodecyl alcohol polyoxyethylene ether sodium sulfate, trimethyl bromination
Ammonium, methyl 2- hydroxy-isobutyric acid ester, the volume ratio of 3- methoxy methyl propionate, 1- methoxy-2-propanol ester, ethyl acetate, water
Example is 1:2:2:1:2:15:50.
<Comparative example 1>
Low alkali high temperature and pressure decomposes wolframite and prepares the method for coarse sodium tungstate with embodiment 3, wherein different
It is 180 DEG C of the decomposition temperature of wolframite mixing slurry.
<The resolution ratio of wolframite is evaluated>
The filter residue that is obtained after pressure filtration washing of wolframite mixing slurry after being decomposed using in Examples 1 to 3 and comparative example 1 as
Evaluation object measures the content of tungstic acid in filter residue, calculates the resolution ratio of wolframite.
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | |
| The content % of tungstic acid | 1.12 | 1.5 | 0.9 | 3.84 |
| Resolution ratio % | 99.59 | 99.42 | 99.68 | 98.51 |
Examples 1 to 3 and comparative example 1 the result shows that, the height of decomposition temperature has obviously the decomposition of tungsten in black tungsten essence
Influence, after will not changing wolframite and decomposing ingredient situation at a temperature of, decomposition temperature Gao Yuegao, tungsten in wolframite
Resolution ratio is higher.
<The evaluation of organic impurities in sodium tungstate solution>
Using coarse sodium tungstate obtained in embodiment 3 and embodiment 4 as evaluation object, measure in coarse sodium tungstate
Organic impurities, there are 12 visible impurity peaks in the coarse sodium tungstate in embodiment 3, occur in embodiment 44 it is visible
Impurity peaks, wolframite powder is through neopelex, polyglyceryl fatty acid ester, ethyl alcohol, water process, and dilution is to decomposition
The processing of wolframite slurry afterwards, reduces organic impurities in coarse sodium tungstate, and coarse sodium tungstate is production ammonium paratungstate
Primary raw material, the organic impurities that the reduction of organic impurities wraps up the ammonium paratungstate product crystallized out in coarse sodium tungstate is more
It is few.
Although the embodiments of the present invention have been disclosed as above, but its is not only in the description and the implementation listed
With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily
Realize other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, the present invention is simultaneously unlimited
In specific details and embodiment shown and described herein.
Claims (7)
1. low alkali high temperature and pressure decomposes the method that wolframite prepares coarse sodium tungstate, which is characterized in that include the following steps：
Wolframite powder and water are mixed to form wolframite slurry, sequentially add sodium hydroxide, tertiary sodium phosphate, sodium nitrate into wolframite slurry
It carries out sizing mixing to form wolframite mixing slurry, wolframite mixing slurry is decomposed, decomposition temperature is 192~210 DEG C, pressure is
0.8~1.0MPa is diluted, filters pressing, washing after decomposition, takes filtrate, obtain coarse sodium tungstate, wherein sodium hydroxide adds
Entering amount is 1.4~1.6 times by the theoretical amount of tungstic acid weight in wolframite powder.
2. low alkali high temperature and pressure as described in claim 1 decomposes the method that wolframite prepares coarse sodium tungstate, feature
It is, granularity is more than or equal to 96% not less than the particle weight accounting of 325 mesh in wolframite slurry.
3. low alkali high temperature and pressure as described in claim 1 decomposes the method that wolframite prepares coarse sodium tungstate, feature
It is, the concentration of sodium hydroxide is 175~200g/L in wolframite mixing slurry, the concentration of tertiary sodium phosphate is 20~65g/L, nitric acid
The concentration of sodium is 5~10g/L.
4. low alkali high temperature and pressure as described in claim 1 decomposes the method that wolframite prepares coarse sodium tungstate, feature
It is, mixing speed control is 70~75r/min, 3~4h of heat-insulation pressure keeping in decomposable process.
5. low alkali high temperature and pressure as claimed in claim 2 decomposes the method that wolframite prepares coarse sodium tungstate, feature
Be, it is diluted the specific steps are：Into dilution trap, note 1/3 dilutes the water of sump volume, then mixes the wolframite after decomposition
Slurry imports in dilution trap.
6. low alkali high temperature and pressure as described in claim 1 decomposes the method that wolframite prepares coarse sodium tungstate, which is characterized in that
Time of filter pressing is 25~30min, and the temperature of slurry is 50~60 DEG C.
7. low alkali high temperature and pressure as claimed in claim 5 decomposes the method that wolframite prepares coarse sodium tungstate, feature
It is, the preparation method of wolframite powder is：Choose the wolframite collocation of the wolframite and low calcium content of high calcium content
The wolframite that total calcium content is not more than 2% is formed, wolframite is taken to be broken into wolframite particle, by superfine mill and sieve
Extension set forms closed circuit, takes wolframite particle to be added in superfine mill and is milled, is delivered to solid material delivery pump
It is sieved in screening machine, screenings flows into pulp tank from diversion trench, and when oversize accumulation is more, the compass screen surface of screening machine is tilted
By oversize from diversion trench import superfine mill, after screening, into pulp tank be added neopelex, gather it is sweet
Oil and fat acid esters, ethyl alcohol, water, ultrasound, filter to take filter residue, dry, obtain wolframite powder, wherein neopelex,
Polyglyceryl fatty acid ester, ethyl alcohol, water volume ratio be 1:2:15:100；By the wolframite mixing slurry after decomposition in dilution
Import after dilution trap and be additionally added dilution, be passed through 400~500mL/min of nitrogen from dilution trench bottom, then with ethyl acetate into
Row extraction, oscillation, stratification remove organic layer solution, carry out filters pressing to water layer solution, wherein dilution includes：Propylene glycol
Alkylether acetates, dodecyl alcohol polyoxyethylene ether sodium sulfate, dodecyl trimethyl ammonium bromide, methyl 2- hydroxy-iso-butyric acid
Ester, 3- methoxy methyl propionate, 1- methoxy-2-propanol ester, ethyl acetate, water, wherein propylene glycol alkyl ether acetic acid ester, ten
Dialkyl group alcohol polyethenoxy ether sodium sulfate, dodecyl trimethyl ammonium bromide, methyl 2- hydroxy-isobutyric acid ester, 3- methoxypropionic acid
Methyl esters, 1- methoxy-2-propanol ester, ethyl acetate, water volume ratio be 1:2:2:1:2:15:50.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810813445.XA CN108913884B (en) | 2018-07-23 | 2018-07-23 | Method for preparing crude sodium tungstate solution by decomposing wolframite concentrate at low alkali and high temperature and pressure |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810813445.XA CN108913884B (en) | 2018-07-23 | 2018-07-23 | Method for preparing crude sodium tungstate solution by decomposing wolframite concentrate at low alkali and high temperature and pressure |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108913884A true CN108913884A (en) | 2018-11-30 |
| CN108913884B CN108913884B (en) | 2019-12-17 |
Family
ID=64417062
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810813445.XA Expired - Fee Related CN108913884B (en) | 2018-07-23 | 2018-07-23 | Method for preparing crude sodium tungstate solution by decomposing wolframite concentrate at low alkali and high temperature and pressure |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108913884B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109439929A (en) * | 2018-12-17 | 2019-03-08 | 江西理工大学 | A kind of method that alkaline system decomposes Scheelite-Wolframite Mixed Mine |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86100031A (en) * | 1986-01-07 | 1986-09-10 | 中国科学院化工冶金研究所 | The treatment process of calcareous tungsten ore material |
| CN1410562A (en) * | 2002-04-10 | 2003-04-16 | 株洲硬质合金集团有限公司 | United decomposition technology of tungstite, wolframite alkali decomposition |
| CN1730686A (en) * | 2005-08-15 | 2006-02-08 | 郴州钻石钨制品有限责任公司 | Method of combined dissolve to multiple tungsten to deeply extracting tungsten |
| CN101643245A (en) * | 2008-08-05 | 2010-02-10 | 江西稀有稀土金属钨业集团有限公司 | Process for preparing high-purity ammonium paratungstate |
| CN104263975A (en) * | 2014-10-09 | 2015-01-07 | 江西稀有金属钨业控股集团有限公司 | Metallurgical technology with multiple closed cycles for tungsten mineral raw materials |
| CN104805314A (en) * | 2015-05-13 | 2015-07-29 | 中南大学 | Method for extracting tungsten from raw materials containing wolframite |
| CN105413855A (en) * | 2015-12-30 | 2016-03-23 | 中南大学 | Method for cleaning and purification of tungsten rough concentrate |
| CN106423573A (en) * | 2016-10-28 | 2017-02-22 | 江西理工大学 | Application method of ester-based hydroximic acid collecting agent to mineral flotation |
-
2018
- 2018-07-23 CN CN201810813445.XA patent/CN108913884B/en not_active Expired - Fee Related
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86100031A (en) * | 1986-01-07 | 1986-09-10 | 中国科学院化工冶金研究所 | The treatment process of calcareous tungsten ore material |
| CN1410562A (en) * | 2002-04-10 | 2003-04-16 | 株洲硬质合金集团有限公司 | United decomposition technology of tungstite, wolframite alkali decomposition |
| CN1730686A (en) * | 2005-08-15 | 2006-02-08 | 郴州钻石钨制品有限责任公司 | Method of combined dissolve to multiple tungsten to deeply extracting tungsten |
| CN101643245A (en) * | 2008-08-05 | 2010-02-10 | 江西稀有稀土金属钨业集团有限公司 | Process for preparing high-purity ammonium paratungstate |
| CN104263975A (en) * | 2014-10-09 | 2015-01-07 | 江西稀有金属钨业控股集团有限公司 | Metallurgical technology with multiple closed cycles for tungsten mineral raw materials |
| CN104805314A (en) * | 2015-05-13 | 2015-07-29 | 中南大学 | Method for extracting tungsten from raw materials containing wolframite |
| CN105413855A (en) * | 2015-12-30 | 2016-03-23 | 中南大学 | Method for cleaning and purification of tungsten rough concentrate |
| CN106423573A (en) * | 2016-10-28 | 2017-02-22 | 江西理工大学 | Application method of ester-based hydroximic acid collecting agent to mineral flotation |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109439929A (en) * | 2018-12-17 | 2019-03-08 | 江西理工大学 | A kind of method that alkaline system decomposes Scheelite-Wolframite Mixed Mine |
| CN109439929B (en) * | 2018-12-17 | 2020-07-28 | 江西理工大学 | Method for decomposing wolframite and wolframite mixed ore by alkaline system |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108913884B (en) | 2019-12-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105253867B (en) | A kind of production method of phosphoric acid by wet process by-product αsemiwatergypsum | |
| CN104495927B (en) | Prepare the method for Vanadium Pentoxide in FLAKES | |
| CN101850992A (en) | Method for preparing calcium carbonate and co-producing sodium sulfate by using phosphorus gypsum and soda ash | |
| CN103787372A (en) | Method for extracting potassium chloride from high-silt-content high-grade feldspar salt mine | |
| CN107419335A (en) | The method that hydrochloric acid method Cycle-decomposition ardealite and phosphorus mine tailing prepare calcium sulfate crystal whiskers | |
| CN107162019A (en) | A kind of processing method of carnallite | |
| CN108707765A (en) | A kind of method that scheelite is decomposed in the pressurization of phosphorus sulphur nitration mixture | |
| CN109573972A (en) | A kind of method of mid low grade phosphate rock production phosphoric acid and low silica cream | |
| CN110028084A (en) | A method of the potassium chloride rate of recovery is improved using mine water | |
| CN114653473B (en) | Flotation method for efficiently purifying phosphogypsum | |
| CN108913884A (en) | Low alkali high temperature and pressure decomposes the method that wolframite prepares coarse sodium tungstate | |
| CN105925797A (en) | Method and system for decomposing scheelite concentrate | |
| CN109174460A (en) | A kind of method for floating of cassiterite | |
| CN102653407B (en) | Method for preparing potassium chloride from sulfate type salt lake brine | |
| CN102659153A (en) | Improvement of aluminium hydroxide production process technology | |
| CN104263973A (en) | Method for preparing APT (Ammonium Paratungstate) from tungsten mineral raw material by multiple closed loops | |
| CN112591782B (en) | Conversion and purification method of low-consumption dihydrate phosphogypsum | |
| CN106319212A (en) | Method for resolving scheelite at normal pressure in alkaline system | |
| CN104743580A (en) | Method for extracting and recycling residual potassium chloride from salt-lake tail salt and waste carnallite | |
| CN112813275A (en) | Method for inhibiting reaction loss of metal aluminum in aluminum ash wet-process aluminum extraction process | |
| CN104263975A (en) | Metallurgical technology with multiple closed cycles for tungsten mineral raw materials | |
| CN107827114A (en) | The method of phosphorus co-production dihydrate gypsum and prodan in recovery wet-process phosphoric acid concentration slag acid | |
| CN102602979A (en) | Preparation method for copper chloride hydroxide | |
| CN103708504B (en) | Utilize the method for mixed potassium salt mine preparing potassium chloride | |
| CN102560158A (en) | Transformation method for mixed rare earth concentrate and concentrated sulfuric acid low-temperature roasted ore |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20191217 Termination date: 20210723 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |